CN1816590A - Silane formulation with high filler content - Google Patents

Silane formulation with high filler content Download PDF

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Publication number
CN1816590A
CN1816590A CN200480019036.9A CN200480019036A CN1816590A CN 1816590 A CN1816590 A CN 1816590A CN 200480019036 A CN200480019036 A CN 200480019036A CN 1816590 A CN1816590 A CN 1816590A
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preparation
alkyl
component
silicomethane
weight
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CN1816590B (en
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R·伊德曼恩
B·博鲁普
C·瓦斯梅
J·蒙基维茨
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Evonik Operations GmbH
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Degussa GmbH
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3081—Treatment with organo-silicon compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3684—Treatment with organo-silicon compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40—Compounds of aluminium
    • C09C1/407—Aluminium oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability

Abstract

The present invention relates to a formulation comprising (i) at least one organoalkoxysilane and/or at least one organoalkoxysiloxane and (ii) at least one inorganic oxidic powder and (iii), if desired, an organic or inorganic acid, component (ii) making up from 5 to 50% by weight of formulation, and the formulation having a viscosity of less than 1500 mPa-s. The present invention further relates to a process for preparing such formulations, and to their use.

Description

Silane formulation with high filler content
The present invention relates to comprise the organoalkoxysilane and the new preparation of inorganic oxide powder at high proportion, its preparation and application thereof.
In many chemical productss, inorganic oxide powder is used as the pigment of colouring application and is used as filler.The example comprises silicon-dioxide or the corresponding titanium dioxide or the aluminum oxide of pyrolysis method preparation, precipitated alumina or oxide hydroxide or aluminium hydroxide, precipitated silica, ferric oxide, zirconium white and other metal oxide.Described powder is used to the preparation of plastics for example and paint and ink.The problem here is that powder particle should be distributed in the product as far as possible equably.Silane also is often used in the preparation of such product.Its surface also can be used with the powder that silane carries out modification.And the homogeneity of ion distribution can have substantial influence to the quality of good especially product.With regard to equipment, powder partly is spiked in the composition difficulty normally and effort, and is particularly especially true when particle is very fine.
The purpose of this invention is to provide and to have the other method that little inorganic oxide powder to nanometer range is spiked into organoalkoxysilane.
Realized this purpose according to the present invention described in claims.
Be surprisingly found out that, by sufficient scatter operation, comprise that adding is less than 0.8mol, preferably less than 0.5mol water/silane of mole use and/or the silicon in the siloxanes, can (example comprises wetting ability and hydrophobic pyrogenic silica with nano level inorganic oxide powder, the pyrolysis method aluminum oxide, boehmite and titanium dioxide), particularly with bigger amount, evenly, simply and economically and also more advantageously be admixed to simultaneously in the organic alkoxy siloxanes of the organoalkoxysilane of general formula I and/or general formula I I, compare with the viscosity that only powder is stirred into the preparation of silane and/or siloxanes, the viscosity of system of the present invention significantly reduces.In the preparation of system of the present invention, can also add organic acid or the mineral acid and the wetting aid of catalytic amount.If in its preparation process or use ultrasonication subsequently, can realize the further reduction of system viscosity of the present invention.
The system of the Huo Deing liquid normally clarifying, be clear to lacteous, can be easy to topple over according to the method, described liquid has quite low viscosity and unknown so far very high solids content.
In addition, can be with preparation of the present invention as requested advantageously with organic solvent or for example alcohol or ester dilution of solvent mixture.
In addition, system of the present invention is the liquid of stable storing basically, and it generally has 6-12 month stability in storage in room temperature.
System of the present invention especially is known as high silane formulation of filling hereinafter or is silane formulation or preparation.
Silane formulation of the present invention can be advantageously used for alleged liquid-powder, particularly also can add under the situation of organosilane and/or organo-siloxane.
The present invention is high, and the silane formulation of filling can simply and advantageously use, and especially is applied to derived product, and example is the liquid system of other kind, for example solution, mixture or melt; In this article, compare with the liquid system that powder is spiked into other kind, system of the present invention can by relatively easily, fast and with special homogeneity fusion.
The use of silane formulation of the present invention also is particularly advantageous, because play the hydrolyzable alkoxyl group that solvent action silane still contains enough numbers, it can participate in the condensation reaction with silane or organic OH functional components after further hydrolysis, the organic oxidation composition granule just is admixed in the network when network forms.
Therefore, the invention provides preparation, described preparation comprises (i) at least a organoalkoxysilane and/or at least a organic alkoxy siloxanes, (ii) at least a inorganic oxide powder, (iii) if necessary, organic acid or mineral acid, wherein component (ii) accounts for the 5-50% weight of weight of formulation, preferred 10-35% weight, more preferably 15-32% weight, and very preferred 20-30% weight, and the viscosity that preparation has is less than 1500mPas, preferred 10-800mPas, preferred especially 50-500mPas, very preferably 100-450mPas.
Preparation of the present invention can comprise wetting aid as other component (iv).Operable wetting aid comprises conventional surfactant, particularly Nonoxynol-9, and example is the Marlophen that Sasol produces Product line.
Preparation of the present invention can comprise in addition that (suitable is methyl alcohol or ethanol for thinner v) or solvent, alcohol for example, and if necessary, water as component.
Preparation of the present invention preferably comprises the organoalkoxysilane as at least a general formula (I) of component (i)
R a-Si(OR 1) 4-a (I)，
Wherein R is identical or different, and be straight chain with 1-18 carbon atom,
Ring-type, side chain or the optional alkyl that replaces, preferable methyl, n-propyl or octyl group, the thiazolinyl that perhaps has 2-8 carbon atom, preferred vinyl, perhaps aryl, preferred phenyl, perhaps acryloxyalkyl or methacryloxy alkyl, preferred 3-methacryloxypropyl, perhaps glycidyl oxygen base alkyl, 3-glycidyl oxygen base propyl group for example, perhaps partially fluorinated or fluoridized fluoroalkyl, 13 fluoro-1 for example, 1,2,2-tetrahydrochysene octyl group, perhaps aminoalkyl group, for example the 3-aminopropyl-, N-normal-butyl-3-aminopropyl or N-(2-amino-ethyl)-3-aminopropyl or corresponding single silylanizing or low silylanizing aminoalkyl group, the alkoxyl group that perhaps has 1-6 carbon atom, for example methoxyl group, oxyethyl group, propoxy-or 2-methoxy ethoxy, perhaps urea groups alkyl, perhaps epoxy alkyl, the mercaptoalkyl that perhaps on alkyl, has 1-6 carbon atom, for example 3-sulfydryl propyl group, perhaps silylanizing alkyl sulfane alkyl, for example two [3-(triethoxysilyl) propyl group] four sulfane bases, perhaps thiocyano alkyl, perhaps isocyanato-alkyl, R 1Be straight chain, ring-type or the straight chained alkyl with 1-6 carbon atom, preferable methyl, ethyl or n-propyl or sec.-propyl, a are 0 or 1 or 2,
And/or the organic alkoxy siloxanes of at least a general formula (II)
R 2 R 3 x ( R 4 - O ) y Si O ( 3 - x - y ) 2 - - - ( II )
Radicals R wherein 2Be identical or different, and R 2Be the alkyl of straight chain, ring-type, side chain or replacement, have the thiazolinyl of 2-8 carbon atom, aryl with 1-18 carbon atom, acryloxyalkyl or methacryloxy alkyl, glycidyl oxygen base alkyl, epoxy alkyl, fluoroalkyl, aminoalkyl group, silylanizing aminoalkyl group, the urea groups alkyl, the mercaptoalkyl that in alkyl, has 1-6 carbon atom, silylanizing alkyl alkylthio base, thiocyano alkyl, isocyanato-alkyl or have the alkoxyl group of 1-6 carbon atom, R 3Be the alkyl of straight chain, ring-type, side chain or replacement with 1-18 carbon atom, R 4Be straight chain, ring-type or the branched-chain alkyl with 1-6 carbon atom, x is 0 or 1 or 2, and y is 0 or 1 or 2, and condition is (x+y)＜3.
And preparation of the present invention preferably comprises at least a nanoscale powder (ii), the mean particle size (d that described powder has 50) less than 1200nm, be preferably 50-1000nm, more preferably 100-900nm very preferably is 200-800nm, such powder preferably is selected from silicon oxide, for example Aerosil , aluminum oxide, for example aluminum oxide C, and titanium oxide.The fineness of grinding as determining according to DIN EN ISO 1524 usefulness grindometers, is generally＜10 μ m.Size-grade distribution can be determined by laser diffraction.
In addition, preparation of the present invention can comprise component (i) and at least a reaction product (ii) as other component, in this case, according to model concept, the component (i) of component (i) or partial hydrolysis if appropriate can with at powder lip-deep reactive center (ii) hydroxyl reaction for example, eliminate pure molecule or water molecules simultaneously.
According to DIN/ISO 3251 " varnish, the mensuration of non-volatile part of painting and being used for the tackiness agent of varnish and paint " (aptly in 125 ℃ kiln 1 hour), preparation of the present invention can advantageously have and is up to 90% weight, preferably be up to 80% weight, the solids content that very preferably is up to 60% weight, based on the weight of formulation meter, each components total 100% weight of preparation.
The present invention also provides the method for preparing preparation, although described preparation has the highly filled low viscosity that has, described method comprises
-with component (i), (iv) mix (ii) and if necessary,
-add 0.001 silicon to＜0.8mol water/molar constituent (i), silicon in preferred 0.05-0.5mol water/molar constituent (i), the more preferably silicon in 0.1-0.4mol water/molar constituent (i), the silicon in 0.2-0.35mol water/molar constituent (i) very preferably, add together if necessary catalytic amount according to component (iii) organic acid or mineral acid and
-mixture is fully disperseed.
Organoalkoxysilane as general formula (I), the preferred methyl-triethoxysilane of using, methyl trimethoxy oxygen base silicomethane, n-propyl trimethoxy silicomethane, the n-propyl triethoxy-silicane, the vinyl triethoxyl silicomethane, the vinyl trimethoxy silicomethane, 3-methacryloxypropyl trimethoxy silicomethane, 3-methacryloxypropyl triethoxy-silicane, 3-glycidyl oxygen base propyl trimethoxy silicomethane, 3-glycidyl oxygen base propyl triethoxy silicomethane, 13 fluoro-1,1,2,2-tetrahydrochysene octyl group trimethoxy silicomethane, 13 fluoro-1,1,2,2-tetrahydrochysene octyl group triethoxy-silicane, 3-aminopropyl trimethoxy silicomethane, N-(normal-butyl)-3-aminopropyl trimethoxy silicomethane, N-(2-amino-ethyl)-3-aminopropyl trimethoxy silicomethane, N-(2-amino-ethyl)-3-aminopropyl methyl dimethoxy oxygen base silicomethane, two (3-trimethoxy-silylpropyl) amine, 3-sulfydryl propyl trimethoxy silicomethane, the organic alkoxy siloxanes of perhaps at least a general formula (II), the organic alkoxy siloxanes that perhaps is selected from aminosilane with according to DE 101 51 264 and mixture alkyl silane and/or organofunctional silane, 3-methacryloxypropyl trimethoxy silicomethane and mixture according to the alkyl silane of DE 198 34 990 etc., alkyl silane and mixture according to the alkyl silane of EP 0 978 525 A2 or EP0 814 110 A1, especially the mixture of methyl trialkoxysilane and propyl trialkoxy silane or phenyl trialkoxy silane, and vinyl alkoxy silane and according to the mixture of the alkylalkoxy silane of EPO 0 518057 A1, alkoxyl group is methoxy or ethoxy preferably, perhaps the mixture of the organic alkoxy siloxanes of the organoalkoxysilane of general formula (I) and general formula (II).
In the methods of the invention, the preferred use is selected from following nanoscale powder as component (ii): silicon oxide, for example pyrogenic silica, precipitated silica, silicate, pure aluminium silicate, aluminum oxide, comprise oxide hydroxide or aluminium hydroxide, transition metal oxide, for example titanium oxide, metatitanic acid, ferric oxide, zinc oxide, cupric oxide, chromic oxide or their mixture preferably have 50-400m according to (ii) powder 2The BET surface-area of/g.As an example but be not to get rid of other, can use silicon-dioxide in the methods of the invention, for example derive from the Aerosil of Degussa 380, preferably have 380m 2The BET surface-area of/g, aluminum oxide for example derive from the boehmite Disperal of Sasol Germany GmbH P3 preferably has 300m 2The BET surface-area of/g derives from the aluminum oxide C of Degussa, preferably has 100m 2The BET surface-area of/g, and titanium dioxide for example derive from the RM 300 of Sachtleben, preferably have 80m 2The BET surface-area of/g.
In the methods of the invention, with component (i) and (ii) suitable to 19: 1-1: 1, preferred 10: 1-3: 2 part by weight uses.
As component (iii), preferred organic acid or mineral acid, preferred hydrogenchloride, form with for example moisture or spissated hydrochloric acid, perhaps formic acid, acetate, vinylformic acid, toxilic acid or other suitable organic acid, described acid with 10-3500ppm weight, preferred 100-1000ppm weight, more preferably the amount of 200-400ppm weight exists, based on (i) amount meter of component in the preparation.
The inventive method is preferably carried out in dispersing apparatus.The preferred dispersing apparatus that uses with good shearing action.On laboratory scale, for example can use, for example the dissolver of Dispermat CV or Ultra-Turrax T 25 types.
Preferably under 0-80 ℃, preferred 10-60 ℃ of temperature, disperseing 10-60 minute, more preferably 15-40 minute of employed component.
The dispersion that obtains in this way or preparation can be stirred under 30-80 ℃ of temperature and carry out aftertreatment in 1-8 hour, preferred 2-6 hour.
By adding organic acid or mineral acid, preparation of the present invention can be adjusted to pH 2-7, preferred pH 3-5.According to the present invention, using under the situation of aminosilane, pH generally is by the character decision of the aminosilane that uses, and is in usually in the alkaline range, certainly by adding acid preparation is become neutrality or acidity.
The present invention also provides the preparation that obtains by the inventive method.
According to the present invention, preparation of the present invention or suitable dilution can be used for anti-scratch trace application, wear-resistant application, protection against corrosion application, application easy to clean, barrier use, be used for the electronics segmentation, be used for circuit board surface handle, as insulation layer, as releasing layer, be used for the top coat of solar cell, as glass fiber size and be used for nanoscale powder evenly is admixed in other kind system.
Can be particularly advantageous in the preparation of plastics, tackiness agent, sealing agent, ink and paint by the preparation that the present invention is such, and be used for the synthetic of resin-based materials.
Therefore, the present invention also provides preparation of the present invention to be used for the synthetic resins sill, perhaps as the component in plastics, tackiness agent, sealing agent, ink and the paint, and the application of the component in perhaps preparing as their.
The present invention also provides the article that can use preparation of the present invention and obtain.
In general, the inventive method can followingly be carried out:
Usually, with component (i), (ii), (iii) and/or (iv) with the hydration of pre-metering also, and mixture disperseed to produce uniformly mobile preparation easily.Also can be by adding component (the preparation dilution that v) will obtain in this way; That is to say, solvent or thinner can be added in the preparation of the present invention, preferably give alcohol (v) as component, for example methyl alcohol, ethanol, Virahol, butanols, 2-methoxypropanol, glycol is butyl glycol, propyl group glycol, glycol ethers for example, and aromatic hydrocarbons is dimethylbenzene, toluene for example, and ester is ethyl acetate, butylacetate for example, ketone is methyl ethyl ketone for example, perhaps their mixture.Surprisingly, also can water as thinner, particularly when glycidyl oxygen yl alkyl alkoxy silane is used as component (i).
Also find, with the preparation of the inventive method preparation with processor for ultrasonic wave for example UP 200 S carry out aftertreatment, can advantageously cause the further reduction of viscosity and the further improvement of particle fineness.
By the following examples the present invention is illustrated:
Embodiment
Embodiment 1
At DYNASYLAN The Aerosil of 30% weight among the MTES 380
With 90.0g methyl-triethoxysilane (DYNASYLAN MTES) place 250ml stainless steel dispersion cups, and under agitation (Dispermat CV) adds the solution of 2.7g deionized water and 0.05g concentrated hydrochloric acid with two covers.With the circumferential speed of water-cooled while liquid was stirred in dissolver 5 minutes with 0.8m/s.That continues begins to add the nano level pyrogenic silica (Aerosil of 40g 380).When the Aerosil of 4-5% weight was distributed in the hydrolysate, viscosity obviously increased.Further adding in the process of Aerosil, the speed of dissolver is being increased to gradually the circumferential speed of about 8m/s.Blending time is approximately 15 minutes.After all Aerosil adds fully, will disperse immediately to proceed 3 minutes with the circumferential speed of 25m/s.In the process of scatter operation, temperature is risen to 38 ℃.The liquid that will so obtain was in 80 ℃ of restir 2 hours subsequently.
So just obtain pale yellowish opalescent liquid, described liquid is measured in 20 ℃ (DIN 53015) has the viscosity of about 400mPas.Isolate a part of liquid, and it is used processor for ultrasonic wave UP 200S aftertreatment 3 minutes, consequently viscosity drop is to about 130mPas (DIN53015).
In 50 ℃ of storages 12 months, system kept stable and does not observe tangible precipitation with this product.
According to DIN/ISO 3251, the solids content of measuring products therefrom is 40% of a composition weight.UV transmission plot (1cm silica glass cuvette is measured facing to air) indication is at 200-250nm zone internal transmission factor＜2%.
Embodiment 2
At DYNASYLAN The Aerosil of 20% weight among the VTMO 380
With 90.0g vinyl trimethoxy silicomethane (DYNASYLAN VTMO) place in the 250ml stainless steel dispersion cup, and under agitation (Dispermat CV) adds the solution of 3.3g deionized water and 0.05g concentrated hydrochloric acid.With the circumferential speed of water-cooled while liquid was being stirred in dissolver 5 minutes with 0.8m/s.That continues begins to add the nano level pyrogenic silica (Aerosil of 31.2g 380).When the Aerosil of 4-5% weight was distributed in the hydrolysate, viscosity obviously increased.Further adding in the process of Aerosil, the speed of dissolver is being increased to gradually the circumferential speed of about 8m/s.Blending time is approximately 20 minutes.At whole Aerosil After adding fully, will disperse immediately to proceed 3 minutes with the circumferential speed of 25m/s.In the process of scatter operation, temperature is risen to 41 ℃.The liquid that will so obtain was in 65 ℃ of restir 2 hours subsequently.
Obtain clarification, weak yellow liquid like this, described liquid is in 20 ℃ of mensuration (DIN 53015) viscosity＜1000mPas.In 50 ℃ of storages 12 months, system kept stable and does not observe tangible precipitation with product.
According to DIN/ISO 3251, the solids content of measuring products therefrom is 42% of a composition weight.
Embodiment 3
At DYNASYLAN The Aerosil of 30% weight among the MEMO 380
With 90.0g 3-methacryloxypropyl trimethoxy silicomethane (DYNASYLAN MEMO) place 250ml stainless steel dispersion cup, and under agitation (Dispermat CV) adds the solution of 2.0g deionized water and 0.3g vinylformic acid and 10.0g methyl alcohol.Simultaneously liquid circumferential speed with 0.8m/s in dissolver was being stirred 5 minutes with water-cooled.That continues begins to add the nano level pyrogenic silica (Aerosil of 43.5g 380).When the Aerosil of 4-5% weight was distributed in the hydrolysate, viscosity obviously increased.Further adding in the process of Aerosil, the speed of dissolver is being increased to gradually the circumferential speed of about 8m/s.Blending time is approximately 22 minutes.At whole Aerosil After adding fully, will disperse immediately to proceed 3 minutes with the circumferential speed of 25m/s.In the process of scatter operation, temperature is risen to 35 ℃.The liquid that will so obtain was in 64 ℃ of restir 2 hours subsequently.
Obtain clarification, colourless liquid like this.In 50 ℃ of storages 3 months, system kept stable and does not observe tangible precipitation with product.
According to DIN/ISO 3251, the solids content of measuring products therefrom is 80% of a composition weight.
Embodiment 4
At DYNASYLAN The Aerosil of 20% weight among the DAMO 380
90.0g N-(2-amino-ethyl)-3-aminopropyl trimethoxy silicomethane (DYNASYLAN DAMO) place 250ml stainless steel dispersion cup.Stir (Dispermat CV) and begin to add the nano level pyrogenic silica (Aerosil of 23.0g simultaneously with the circumferential speed of 0.8m/s with water-cooled 380).When the Aerosil of 4-5% weight was distributed in the hydrolysate, viscosity obviously increased.Further adding in the process of Aerosil, the speed of dissolver is being increased to gradually the circumferential speed of about 8m/s.Blending time is approximately 10 minutes.At whole Aerosil After adding fully, will disperse immediately to proceed 3 minutes with the circumferential speed of 25m/s.In the process of scatter operation, temperature is risen to 37 ℃.
Obtain clarification, lacteous liquid like this.In 50 ℃ of storages 12 months, system kept stable and does not observe tangible precipitation with product.
According to DIN/ISO 3251, the solids content of measuring products therefrom is 81% of a composition weight.
Embodiment 5
At DYNASYLAN The aluminum oxide C of 17% weight among the AMMO
90.0g 3-aminopropyl trimethoxy silicomethane (DYNASYLAN AMMO) place 250ml stainless steel dispersion cup, under agitation (Dispermat CV) adds the 7.2g deionized water.With the circumferential speed of water-cooled while liquid was stirred in dissolver 5 minutes with 0.8m/s.The beginning that continues adds 23g nano level pyrolysis method aluminum oxide (aluminum oxide C) under the circumferential speed of 0.8m/s.When the aluminum oxide of 4-5% weight was distributed in the hydrolysate, viscosity obviously increased.Further adding in the process of aluminum oxide, the speed of dissolver is being increased to gradually the circumferential speed of about 8m/s.Blending time is approximately 10 minutes.After all aluminum oxide adds fully, will disperse immediately to proceed 3 minutes with the circumferential speed of 25m/s.In the process of scatter operation, temperature is risen to 34 ℃.
Obtain oyster white, opalescent liquid like this, described liquid is in 20 ℃ of mensuration (DIN 53015) viscosity＜10000mPas.In 50 ℃ of storages 4 months, system kept stable and does not observe tangible precipitation with product.
Embodiment 6
At DYNASYLAN The Aerosil of 26% weight in 1189 380
400.0g N-(normal-butyl)-3-aminopropyl trimethoxy silicomethane (DYNASYLAN 1189) place 1 liter of stainless steel dispersion cup, and under agitation (Dispermat CV) adds the 9.15g deionized water.With the circumferential speed of water-cooled while liquid was being stirred in dissolver 5 minutes with 0.8m/s.The beginning that continues adds the nano level pyrogenic silica (Aerosil of 127g under the circumferential speed of 0.8m/s ).When the Aerosil of 4-5% weight was distributed in the hydrolysate, viscosity obviously increased.Further adding in the process of Aerosil, the speed of dissolver is being increased to gradually the circumferential speed of about 8m/s.Blending time is approximately 45 minutes.At whole Aerosil After adding fully, will disperse immediately to proceed 5 minutes with the circumferential speed of 25m/s.Dispersion temperature is risen to 56 ℃.Obtain flaxen clarified liq like this.
Subsequently, at 60 ℃ of bath temperatures and P DefinitelyUnder=1 millibar the condition, by the high Silan-Aerosil that fills of evaporation in Rotary Evaporators Preparation is removed the 54g methyl alcohol that is discharged by hydrolysis.Dense Silane-Aerosil Free methanol content (GC)＜1% in the preparation.This clear, pale yellowish liquid has the viscosity of 309mPas 20 ℃ (DIN 53015).
In 50 ℃ of storages 2 months, system kept stable and does not observe tangible precipitation during this period with product.
Embodiment 7
At DYNASYLAN The titanium dioxide of 10% weight among the GLYMO
400.0g 3-glycidyl oxygen base propyl trimethoxy silicomethane (DYNASYLAN GLYMO) place 250ml stainless steel dispersion cup, and under agitation (DispermatCV) adds 20g ethanol and 20g titanium dioxide water-dispersion liquid (RM 300 WP, TiO 2Content is 37.8% weight, derives from Sachtleben).With the circumferential speed of water-cooled while, liquid was stirred in dissolver 5 minutes with 1.0m/s.With polymeric amide cover synusia change dissolver sheet, and add the zirconium oxide abrasive pearl of 80ml d=0.7-1.2mm thereafter.Use the pearl of grinding thus with silane-TiO 2Preparation aftertreatment 20 minutes.In the scatter operation process, temperature is risen to 43 ℃.
Obtain having d like this 50The milky white cream-coloured opalescent liquid of the average particle size distribution of=80nm (by determination of laser diffraction).
In 50 ℃ of storages 6 months, system kept stable during this period, does not significantly precipitate with this product.
Embodiment 8
At DYNASYLAN The Aerosil of 22% weight among the GLYMO 380
60.0g 3-glycidyl oxygen base propyl trimethoxy silicomethane (DYNASYLAN GLYMO) place 250ml stainless steel dispersion cup, and under agitation (DispermatCV) adds the solution of 10.0g deionized water and 0.1g spirit acid.Circumferential speed with 0.8m/s stirred liquid 5 minutes in dissolver.That continues begins to add the nano level pyrogenic silica (Aerosil of 20.0g 380).Aerosil when 4-5% weight When being distributed in the hydrolysate, viscosity obviously increases.Further adding Aerosil Process in, the speed of dissolver is increased to gradually the circumferential speed of about 8m/s.Blending time is approximately 12 minutes.At whole Aerosil After adding fully, will disperse immediately to proceed 2 minutes with the circumferential speed of 25m/s.Dispersion temperature in the uncooled container is risen to 28 ℃.
Had like this＜the clarifying shallow opalescent liquid of the viscosity of 1000mPas.Silane formulation is mixed with 50% deionized water, obtain low viscous opalescent liquid.In 50 ℃ of storages 1 month, system kept stable during this period with this product, and did not significantly precipitate.
With 6 μ m scalpels the aqueous silane preparation is applied to be coated with aluminium sheet (3105 H24 alloy), coating in 200 ℃ of dryings 15 minutes.Transparent coating shows good anti-Steel Wool scraping.
Embodiment 9
At DYNASYLAN The Aerosil of 25% weight among the VTMO R972
170.0g vinyl trimethoxy silicomethane (DYNASYLAN VTMO) place 500ml stainless steel dispersion cup, and under agitation (Dispermat CV) adds the solution of 6.2g deionized water and 0.18g concentrated hydrochloric acid.Circumferential speed with 0.8m/s stirred liquid 5 minutes in dissolver.That continues begins to add 50.0g nano level hydrophobic fumed silica (Aerosil R972).Aerosil when 4-5% weight When being distributed in the hydrolysate, viscosity obviously increases.Further adding Aerosil Process in, the speed of dissolver is increased to gradually the circumferential speed of about 8m/s.Blending time is approximately 21 minutes.At whole Aerosil After adding fully, will disperse immediately to proceed 5 minutes with the circumferential speed of 25m/s.Dispersion temperature in the uncooled container is risen to 39 ℃.
Obtain having the pale yellowish opalescent liquid of the viscosity of 535mPas like this.
In 50 ℃ of storages 12 months, system kept stable during this period, and does not observe tangible precipitation with this product.
Comparing embodiment
At DYNASYLAN The Aerosil of 8% weight among the MTES 380
90.0g methyl-triethoxysilane (DYNASYLAN MTES) place 250ml stainless steel dispersion cup.That continues mixes 8g nano level pyrogenic silica (Aerosil immediately 380).Add 5g Aerosil 380 back viscosity significantly increase.The speed of dissolver is increased to 8m/s by 0.8m/s, and is metered into 3g Aerosil again 380.Obtain like this starching the sample block, it is removed from dispersion cup with spatula.

Claims (25)

1. the preparation that comprises following component: (i) at least a organoalkoxysilane and/or at least a organic alkoxy siloxanes and (ii) at least a inorganic oxide powder and (iii), if necessary, organic acid or mineral acid, component (ii) accounts for the 5-50% of weight of formulation, and the viscosity of preparation is less than 1500mPas.
2. the preparation of claim 1, described preparation comprises as other component wetting aid (iv).
3. claim 1 or 2 preparation, described preparation comprises as other component (thinner v) or solvent.
4. each preparation among the claim 1-3, wherein the organoalkoxysilane of component (i) has general formula (I)
R a-Si(OR 1) 4-a (I)，
Wherein radicals R is identical or different, and R is the alkyl of straight chain, ring-type, side chain or replacement with 1-18 carbon atom or the thiazolinyl with 2-8 carbon atom, or aryl, or alkoxyl group, or acryloxyalkyl or methacryloxy alkyl, or epoxy alkyl, or glycidyl oxygen base alkyl, or aminoalkyl group, or fluoroalkyl, or mercaptoalkyl, or silylanizing alkyl sulfane alkyl, or the thiocyano alkyl, or the isocyanato-alkyl, R 1Be straight chain, side chain or cyclic alkyl, and a is 1 or 2 with 1-6 carbon atom.
5. each preparation among the claim 1-4, wherein the organic alkoxy siloxanes of component (i) has general formula (II)
Radicals R wherein 2Be identical or different, and R 2Be the alkyl of straight chain, ring-type, side chain or replacement, have the thiazolinyl of 2-8 carbon atom, aryl with 1-18 carbon atom, acryloxyalkyl or methacryloxy alkyl, glycidyl oxygen base alkyl, epoxy alkyl, fluoroalkyl, aminoalkyl group, silylanizing aminoalkyl group, the urea groups alkyl, mercaptoalkyl, silylanizing alkyl alkylthio base, thiocyano alkyl, isocyanato-alkyl or alkoxyl group, R 3Be the alkyl of straight chain, ring-type, side chain or replacement with 1-18 carbon atom, R 4Be straight chain, ring-type or the branched-chain alkyl with 1-6 carbon atom, x is 0 or 1 or 2, and y is 0 or 1 or 2, and condition is (x+y)＜3.
6. each preparation among the claim 1-5, described preparation comprises the mean particle size (d that has less than 1200nm 50) nanoscale powder (ii).
7. each preparation among the claim 1-6, described preparation comprise be selected from silicon oxide, aluminum oxide and transition metal oxide powder (ii).
8. each preparation among the claim 1-7, described preparation comprise as component of other component (i) and (ii) at least a reaction product.
9. each preparation among the claim 1-8 is characterized in that, solids content is up to 90% weight of weight of formulation, each components total 100% weight of preparation.
10. the method for at least one preparation among the preparation claim 1-9, described method comprises
-with component (i), (iv) mix (ii) and if necessary,
-add 0.001 silicon to＜0.8mol water/molar constituent (i), add together if necessary catalytic amount according to component organic acid or mineral acid (iii), and mixture fully disperseed.
11. the method for claim 10, wherein use be selected from silicon-dioxide, aluminum oxide and transition metal oxide at least a nano grade inorganic powder (ii).
12. the method for claim 10 or 11, wherein use the organoalkoxysilane that is selected from following at least a general formula (I): methyl-triethoxysilane, methyl trimethoxy oxygen base silicomethane, n-propyl trimethoxy silicomethane, the n-propyl triethoxy-silicane, the vinyl triethoxyl silicomethane, the vinyl trimethoxy silicomethane, 3-methacryloxypropyl trimethoxy silicomethane, 3-glycidyl oxygen base propyl trimethoxy silicomethane, 3-glycidyl oxygen base propyl triethoxy silicomethane, 13 fluoro-1,1,2,2-tetrahydrochysene octyl group trimethoxy silicomethane, 13 fluoro-1,1,2,2-tetrahydrochysene octyl group triethoxy-silicane, 3-aminopropyl trimethoxy silicomethane, N-(normal-butyl)-3-aminopropyl trimethoxy silicomethane, N-(2-amino-ethyl)-3-aminopropyl trimethoxy silicomethane, N-(2-amino-ethyl)-3-aminopropyl methyl dimethoxy oxygen base silicomethane, two (3-trimethoxy-silylpropyl) amine or 3-sulfydryl propyl trimethoxy silicomethane.
13. at least one method among the claim 9-12, wherein use the organic alkoxy siloxanes of at least a general formula (II), the perhaps mixture of the organic alkoxy siloxanes of general formula (II), the mixture of the organic alkoxy siloxanes of the organoalkoxysilane of perhaps at least a general formula (I) and general formula (II).
14. at least one method among the claim 9-13 is wherein used the silicon in 0.05-0.5mol water/molar constituent (i).
15. at least one method among the claim 9-14 wherein uses as acid acetate, vinylformic acid or toxilic acid with the amount of 10-3500ppm weight, the amount of described acid is based on the amount meter of the component of using in the preparation (i).
16. at least one method among the claim 9-15, wherein used component are dispersive under 0-80 ℃ of temperature.
17. at least one method among the claim 9-16 is wherein disperseed used component 10-60 minute.
18. at least one method among the claim 9-17 is wherein with thus obtained dispersion or preparation under the 30-80 temperature under agitation aftertreatment 1-8 hour.
19. at least one method among the claim 9-18 wherein is adjusted to pH 2-7 by adding organic acid or mineral acid with preparation.
20. each preparation among the claim 1-8, described preparation can obtain by at least one method among the claim 9-19.
21. the application of at least one preparation or the preparation that makes by each method among the claim 9-19 in claim 1-8 and 20, described application be used for anti-scratch trace application, wear-resistant application, protection against corrosion application, application easy to clean, barrier use, be used for the electronics segmentation, be used for circuit board surface handle, as insulation layer, as releasing layer, be used for the top coat of solar cell, as glass fiber size or be used for nanoscale powder evenly is admixed in other kind system.
22. at least one preparation or the application of preparation in preparation plastics, tackiness agent, sealing agent, resin-based materials, ink or paint that make by each method among the claim 9-19 in claim 1-8 and 20 and 21.
23. at least one preparation or the preparation that makes by each method among the claim 9-19 are as the application of the composition of resin-based materials, plastics, ink, paint, tackiness agent or sealing agent among claim 1-8 and the 20-22.
24. the article that can described in claim 21 or 22, obtain.
25. article described in claim 23 or the article described in claim 24.
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CN1816590B (en) 2010-05-26
US8119730B2 (en) 2012-02-21
US20070110906A1 (en) 2007-05-17
WO2005003218A1 (en) 2005-01-13
EP1641867A1 (en) 2006-04-05
CN101481468A (en) 2009-07-15
JP2009513741A (en) 2009-04-02

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